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Development of a kelp powder (Thallus laminariae) Standard Reference Material

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Abstract

A Standard Reference Material (SRM) of seaweed, SRM 3232 Kelp Powder (Thallus laminariae) has been developed to support food and dietary supplement measurements in compliance with the Food Safety Modernization Act (FSMA) and the Dietary Supplement Health and Education Act of 1994 (DSHEA). The material was characterized for nutritional minerals, arsenic species, isomers of vitamin K1, proximates, and toxic elements. Kelp is a rich source of vitamins and minerals, and it is an excellent source of dietary iodine. Kelp also contains a large amount of arsenic, which is toxic as inorganic species but much less so as organic species. To capture the dietary profile of kelp, certified values were issued for As, Ca, Cd, Cr, Cu, Fe, Hg, I, K, Mg, Mn, Mo, Na, Pb, and Zn. Reference values for proximates were assigned. For the first time, a certified value for iodine, reference values for isomers of vitamin K1, and reference values for arsenic species including arsenosugars were assigned in a seaweed. SRM 3232 fills a gap in Certified Reference Materials (CRMs) needed for quality assurance and method validation in the compositional measurements of kelp and similar seaweeds used as food and as dietary supplements.

Arsenic species and isomers of vitamin K1 were determined in the development of SRM 3232 Kelp Powder (Thallus laminariae).

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References

  1. Wells ML, Potin P, Craigie JS, Raven JA, Merchant SS, Helliwell KE, et al. Algae as nutritional and functional food sources: revisiting our understanding. J Appl Phycol. 2017;29:949–82.

    Article  CAS  Google Scholar 

  2. McHugh DJ. A guide to the seaweed industry. FAO Fisheries Technical Paper 441. Rome: Food and Agriculture Organization of the United Nations; 2003.

  3. Yoshinaga J, Morita M, Yukawa M, Shiraishi K, Kawamura H. Certified reference material for analytical quality assurance of minor and trace elements in food and related matrixes based on a typical Japanese diet: interlaboratory study. J AOAC Int. 2001;84:1202–8.

    CAS  Google Scholar 

  4. Matsumura Y. Nutrition trends in Japan. Asia Pac J Clin Nutr. 2001;10:S40–7.

    Article  Google Scholar 

  5. Brown EM, Allsopp PJ, Magee PJ, Gill CIR, Nitecki S, Strain CS, et al. Seaweed and human health. Nutr Rev. 2014;72:205–16.

    Article  Google Scholar 

  6. Park EJ, Pezzuto JM. Antioxidant marine products in cancer chemoprevention. Antioxid Redox Signal. 2013;19:115–38.

    Article  Google Scholar 

  7. Gupta S, Abu-Ghannam N. Bioactive potential and possible health effects of edible brown seaweeds. Trends Food Sci Technol. 2011;22:315–26.

    Article  CAS  Google Scholar 

  8. Jeménez-Escrig A, Gómez-Ordónez E, Tenorio MD, Rupérez P. Antioxidant and prebiotic effects of dietary fiber co-travelers from sugar Kombu in healthy rats. J Appl Phycol. 2013;25:503–12.

    Article  Google Scholar 

  9. Jensen MG, Petersen C, Kristensen M, Frost G, Astrup A. Review: efficacy of alginate supplementation in relation to appetite regulation and metabolic risk factors: evidence from animal and human studies. Obes Rev. 2013;14:129–44.

    Article  Google Scholar 

  10. MacArtain P, Gill CIR, Brooks M, Camell R, Rowland IR. Nutritional value of edible seaweeds. Nutr Rev. 2007;65:535–43.

    Article  Google Scholar 

  11. Outola I, Filliben J, Inn KGW, LaRosa J, McMahon CA, Peck GA, et al. Characterization of the NIST seaweed standard reference material. Appl Radiat Isot. 2006;64:1242–7.

    Article  CAS  Google Scholar 

  12. Reis PA, Cassiano J, Veiga P, Rubal M, Sousa-Pinto I. Fucus spiralis as monitoring tool of metal contamination in the northwest coast of Portugal under the European Water Framework Directives. Environ Monit Assess. 2014;186:5447–60.

    Article  CAS  Google Scholar 

  13. Mišurcová L, Machů L, Orsavová J. Seaweed minerals as nutraceuticals. Adv Food Nutr Res. 2011;64:371–90.

    Article  Google Scholar 

  14. Narukawa T, Inagaki K, Zhu Y, Kuroiwa T, Narushima I, Chiba K, et al. Preparation and certification of Hijiki reference material, NMIJ CRM 7405-a, from the edible marine algae hijiki (Hizikia fusiforme). Anal Bioanal Chem. 2012;402:1713–22.

    Article  CAS  Google Scholar 

  15. Hijiki: your questions answered. Food Standards Agency, UK. https://www.food.gov.uk/multimedia/hijikiqanda. Cited 8 Oct 2017.

  16. Yvin J-C, LeVasseur F, Hud’Homme F. Use of laminarin and oligosaccharides derived therefrom in cosmetics and for preparing a skin treatment drug. 1999; United States Patent 5,980,916.

  17. Dietary Supplement Health and Education Act of 1994. https://ods.od.nih.gov/About/DSHEA_Wording.aspx#sec6 and Guidance for Industry: Current Good Manufacturing Practice in Manufacturing, Packaging, Labeling, or Holding Operations for Dietary Supplements; Small Entity Compliance Guide December 2010. https://www.fda.gov/food/guidanceregulation/guidancedocumentsregulatoryinformation/dietarysupplements/ucm238182.htm. Cited 8 Oct 2017.

  18. Davis RS. The fourth meeting of the CCQM, February 1998. Accred Qual Assur. 1998;3:502–3.

    Article  Google Scholar 

  19. May W, Parris R, Beck C, Fassett J, Greenberg R, Guenther F, et al. Definitions of terms and modes used at NIST for value assignment of reference materials for chemical measurements. NIST special publication 260–136. Washington, D.C.: US Government Printing Office; 2000.

    Google Scholar 

  20. Sea water quality standard (GB 3097-1997). http://english.mep.gov.cn/standards_reports/standards/water_environment/quality_standard/200710/W020061027511546974673.pdf (in Chinese). http://www.chinesestandard.net/PDF-Excerpt/ShowPDFexcerpt.aspx?ExcerptID=GB%203097-1997 (in English). Cited 8 October 2017.

  21. Long SE, Kelly WR. Determination of mercury in coal by isotope dilution cold-vapor generation inductively coupled plasma mass spectrometry. Anal Chem. 2002;74:1477–83.

    Article  CAS  Google Scholar 

  22. Murphy KE, Beary ES, Rearick MS, Vocke RD. Isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) for the certification of lead and cadmium in environmental standard reference materials. Fresenius J Anal Chem. 2000;368:362–70.

    Article  CAS  Google Scholar 

  23. Murphy KE, Vetter TW. Recognizing and overcoming analytical error in the use of ICP-MS for the determination of cadmium in breakfast cereal and dietary supplements. Anal Bioanal Chem. 2013;405:4579–88.

    Article  CAS  Google Scholar 

  24. Becker DA. 30 years of reactor characterization on the NBSR. J Radioanal Nucl Chem. 2000;244:361–5.

    Article  CAS  Google Scholar 

  25. Greenberg RR, Fleming RF, Zeisler R. High sensitivity neutron activation analysis of environmental and biological Standard Reference Materials. Environ Int. 1984;10:129–36.

    Article  CAS  Google Scholar 

  26. Yu LL, Stanoyevitch RC, Zeisler R. SI traceable determination of arsenic species in kelp (Thallus laminariae). Anal Methods. 2017;9:4267–74.

    Article  CAS  Google Scholar 

  27. Yu LL, Chao W, Zeisler R, Tong J, Oflaz R, Bao H, et al. An approach for identification and determination of arsenic species in the extract of kelp. Anal Bioanal Chem. 2015;407:3517–24.

    Article  CAS  Google Scholar 

  28. Davis WC, Zeisler R, Sieber JR, Yu LL. Methods for the separation and quantification of arsenic species in SRM 2669: arsenic species in frozen human urine. Anal Bioanal Chem. 2010;396:3041–50.

    Article  CAS  Google Scholar 

  29. Otten JJ, Hellwig JP, Meyers LD. Dietary Reference Intakes: The Essential Guide to Nutrient Requirements. Washington, D.C.: National Academies Press; 2006.

    Google Scholar 

  30. JCGM100:2008. Evaluation of Measurement Data—Guide to the Expression of Uncertainty in Measurement (ISO GUM 1995 with Minor Corrections); Joint Committee for Guides in Metrology; available at http://www.bipm.org/utils/common/documents/jcgm/JCGM_100_2008_E.pdf. 2008. Cited 8 October 2017; see also Taylor BN, Kuyatt CE (1994) Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement Results; NIST Technical Note 1297; Washington, DC: U.S. Government Printing Office, available at http://www.nist.gov/pml/pubs/tn1297/index.cfm. Cited 8 October 2017.

  31. JCGM101:2008. Evaluation of Measurement Data – Supplement 1 to the Guide to Expression of Uncertainty in Measurement; Propagation of Distributions Using a Monte Carlo Method; Joint Committee for Guides in Metrology; available at http://www.bipm.org/utils/common/documents/jcgm/JCGM_101_2008_E.pdf. 2008. Cited 8 Oct 2017.

  32. Efron B, Tibshirani RJ. An Introduction to the Bootstrap. London: Chapman & Hall; 1993.

    Book  Google Scholar 

  33. Iodine – Fact Sheet for Health Professionals, National Institute of Health Office of Dietary Supplements. https://ods.od.nih.gov/factsheets/Iodine-HealthProfessional/. Cited 8 Oct 2017.

  34. Oliveira AA, Trevizan LC, Nobrega JA. REVIEW: Iodine determination by inductively coupled plasma spectrometry. Appl Spectrosc Rev. 2010;45:447–73.

    Article  CAS  Google Scholar 

  35. Grindlay G, Mora J, De Loos-Vollebregt M, Vanhaecke F. A systematic study on the influence of carbon on the behavior of hard-to-ionize elements in inductively coupled plasma-mass spectrometry. Spectrochim Acta B. 2013;86:42–9.

    Article  CAS  Google Scholar 

  36. Larsen EH, Ludwigsen MB. Determination of iodine in food-related certified reference materials using wet ashing and detection by inductively coupled plasma mass spectrometry. J Anal At Spectrom. 1997;12:435–9.

    Article  CAS  Google Scholar 

  37. Todorov TI, Gray PJ. Analysis of iodine in food samples by inductively coupled plasma-mass spectrometry. Food Addit Contam Part A. 2016;33:282–90.

    CAS  Google Scholar 

  38. Mesko MF, Costa VC, Picoloto RS, Bizzi CA, Mello PA. Halogen determination in food and biological materials using plasma-based techniques: challenges and trends of sample preparation. J Anal At Spectrom. 2016;31:1243–2161.

    Article  CAS  Google Scholar 

  39. Shelor CP, Dasgupta PK. Review of analytical methods for the quantification of iodine in complex matrices. Anal Chim Acta. 2011;702:16–36.

    Article  CAS  Google Scholar 

  40. Kučera J, Řanda Z, Soukal L. A comparison of three activation analysis methods for iodine determination in foodstuffs. J Radioanal Nucl Chem. 2001;249:61–5.

    Article  Google Scholar 

  41. WHO ten chemicals of major public health concern http://www.who.int/ipcs/assessment/public_health/chemicals_phc/en/ [Cited 8 October 2017] and ATSDR’s Substance Priority List https://www.atsdr.cdc.gov/spl/index.html [Cited 8 October 2017].

  42. EPA Drinking Water Requirements for States and Public Water Systems https://www.epa.gov/dwreginfo/chemical-contaminant-rules [Cited 8 October 2017]. FDA proposes limit for inorganic arsenic in infant rice cereal https://www.fda.gov/NewsEvents/Newsroom/PressAnnouncements/ucm493740.htm [Cited 8 October 2017]. FDA action level for arsenic in apple juice https://www.fda.gov/Food/FoodborneIllnessContaminants/Metals/ucm280209.htm [Cited 8 October 2017].

  43. Amster E, Tiwary A, Schenker MB. Case report: potential arsenic toxicosis secondary to herbal kelp supplement. Environ Health Perspect. 2007;115:606–8. A574–7

    Article  CAS  Google Scholar 

  44. Raab A, Fecher P, Feldmann J. Determination of Arsenic in Algae – Results of an Interlaboratory Trial: Determination of Arsenic Species in the Water-Soluble Fraction. Microchim Acta. 2005;151:153–66.

    Article  CAS  Google Scholar 

  45. Briscoe ML, Ugrai TM, Crewell J, Carter AT. An interlaboratory comparison study for the determination of arsenic and arsenic species in rice, kelp, and apple juice. Spectrosc. 2015;30. http://www.spectroscopyonline.com/print/292389?page=full. Cited 8 Oct 2017.

  46. Gallagher PA, Wei X, Shoemaker JA, Brockhoff CA, Creed JT. Detection of arsenosugars from kelp extracts via IC-electrospray ionization-MS-MS and IC membrane hydride generation ICP-MS. J Anal At Spectrom. 1999;14:1829–34.

    Article  CAS  Google Scholar 

  47. Madsen AD, Goessler W, Pedersen SN, Francesconi KA. Characterization of an algal extract by HPLC-ICP-MS and LC-electrospray MS for use in arsenosugar speciation studies. J Anal At Spectrom. 2000;15:657–62.

    Article  CAS  Google Scholar 

  48. Taylor V, Goodale B, Raab A, Schwerdtle T, Reimer K, Conklin S, et al. Human exposure to organic arsenic species from seafood. Sci Total Environ. 2017;580:266–82.

    Article  CAS  Google Scholar 

  49. Gamble BM, Gallagher PA, Shoemaker JA, Parks AN, Wei X, Schwegel CA, et al. An investigation of the chemical stability of arsenosugars in simulated gastric juice and acidic environments using IC-ICP-MS and IC-ESI-MS/MS. Analyst. 2002;127:781–5.

    Article  CAS  Google Scholar 

  50. Gamble BM, Gallagher PA, Shoemaker JA, Parks AN, Freeman DM, Schwegel CA, et al. An investigation of the chemical stability of arsenosugars in basic environments using IC-ICP-MS and IC-ESI-MS/MS. Analyst. 2003;128:1458–61.

    Article  CAS  Google Scholar 

  51. Yoshinaga J, Shibata Y, Horiguchi T, Morita M. NIES certified reference materials for arsenic speciation. Accred Qual Assur. 1997;2:154–6.

    Article  CAS  Google Scholar 

  52. Van Hulle M, Zhang C, Zhang X, Cornelis R. Arsenic speciation in Chinese seaweeds using HPLC-ICP-MS and HPLC-ES-MS. Analyst. 2002;127:634–40.

    Article  Google Scholar 

  53. Phinney KW, Rimmer CA, Thomas JB, Sander LC, Sharpless KE, Wise SA. Isotope dilution liquid chromatography – mass spectrometry methods for fat- and water-soluble vitamins in nutritional formulations. Anal Chem. 2011;83:92–8.

    Article  CAS  Google Scholar 

  54. Lowenthal J, Vergel Rivera GM. Comparison of the activity of the cis and trans isomer of vitamin K1 in vitamin K-deficient and coumarin anticoagulant- pretreated Rats. J Pharm Exp Ther. 1979;209:330–3.

    CAS  Google Scholar 

  55. Huang B, Zheng F, Fu S, Yao J, Tao B, Ren Y. UPLC-ESI-MS/MS for determining trans- and cis-vitamin K1 in infant formulas: method and applications. Eur Food Res Technol. 2012;235:873–9.

    Article  CAS  Google Scholar 

  56. Lee H, Lee J, Choi K, Kim B. Development of isotope dilution-liquid chromatography/tandem mass spectrometry for the accurate determination of trans- and cis-vitamin K1 isomers in infant formula. Food Chem. 2017;221:729–36.

    Article  CAS  Google Scholar 

  57. Woollard DC, Indyk HE, Fong BY, Cook KK. Determination of vitamin K1 isomers in foods by liquid chromatography with C30 bonded-phase column. J AOAC Int. 2002;85:682–91.

    CAS  Google Scholar 

  58. Greenfield H, Southgate DAT. Food composition data: production, management, and use. 2ed ed. Rome: Food and Agriculture Organization of the United Nations; 2003.

    Google Scholar 

  59. Bender MM, Rader JI, McClure FD. Guidance for Industry: Nutrition Labeling Manual - A Guide for Developing and Using Data Bases. 1998ed. US Food and Drug Administration. https://www.fda.gov/food/guidanceregulation/guidancedocumentsregulatoryinformation/labelingnutrition/ucm063113.htm#N_1_. Cited 8 Oct 2017.

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Acknowledgments

Support for the development of SRM 3232 was provided in part by the Office of Dietary Supplements of the National Institutes of Health (NIH-ODS). A gift of arsenosugar As(328) from Dr. John T. Creed of the U.S. Environmental Protection Agency, National Exposure Research Laboratory in Cincinnati, OH is gratefully acknowledged.

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Yu, L.L., Browning, J.F., Burdette, C.Q. et al. Development of a kelp powder (Thallus laminariae) Standard Reference Material. Anal Bioanal Chem 410, 1265–1278 (2018). https://doi.org/10.1007/s00216-017-0766-z

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